CN101509947A - Electrode for in-situ electrical measurement for diamond anvil cell and method for producing the same - Google Patents
Electrode for in-situ electrical measurement for diamond anvil cell and method for producing the same Download PDFInfo
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Abstract
The invention discloses an in-situ electrical measuring electrode that is used in diamond-pair anvil cells and a manufacturing method thereof, and belongs to the technical field of high-temperature and high-voltage devices. Four electrodes (1) are deposited on the surface of a diamond anvil cell (8) and distribute from an anvil surface to a lateral surface of the diamond anvil cell (8); the electrodes (1) are diamond films doped with boron; a diamond insulating layer (2) covers the anvil surface and the lateral surface of the diamond anvil cell (8) as well as the electrodes (1) thereof; the electrodes (1) are exposed at one end of the anvil surface, the exposed position lies inside a sample cavity (9), and the electrodes (1) are exposed at one end of the lateral surface and connected with an electrode lead (5). A diamond film microcircuit and the diamond insulating layer are simultaneously integrated onto the surface of the diamond anvil cell by utilizing the film deposition technique, the nanometer seeding technique, the masking technique and the photolithographic method. The manufacturing method of the in-situ electrical measuring electrode prevents the electrode from being destroyed by transverse shearing force and overcomes the electrode corrosion by samples under the high-voltage condition, thus widening the research field of electrical in-situ measurement under high voltage.
Description
Technical field
The invention belongs to the technical field of high temperature high pressure device, particularly a kind of boron doped diamond film electrode that is used for original position electric parameter measurement under the adamas opposed anvils high-temperature and high-pressure conditions and preparation method thereof.
Background technology
The adamas opposed anvils is at present uniquely can produce hyperpressure (〉 100GPa) high pressure generating apparatus.Utilize its people to study, and the electrical properties in site measurement of material is exactly one of them important aspect to the variation characteristic of the various physical quantitys of material under the hyperpressure.
Stability has very strict requirement, and promptly 1. electrode can not rupture under high-pressure environment, 2. can not with measured matter generation chemical reaction, 3. can not produce serious deformation.
The mode of metal line is all adopted in high pressure Experiments of Electricity on the early stage adamas opposed anvils, and because sample cavity is very narrow and small, so except the electrode of arranging was very difficult, serious deformation also will take place in electrode itself, at all can't measuring samples resistivity etc. electrical quantities.Introducing along with film deposition techniques and micro-processing technology, people directly are deposited on metal electrode on the adamas anvil face, though solved the problem of electrode deformation, but can only measure the cold sample of solid, in case run into high-temperature and high-pressure conditions, the reaction of metal film electrode and sample can cause electrode failure, causes measuring failure.In addition, metal film electrode still is subjected to the effect of cross shear in anvil face edge, and particularly under hyperpressure, lead rupture still is difficult to avoid.Therefore, inventing and create a kind of intensity high and corrosion resistant electrode preparation and package technique, is the key that thoroughly solves fluent meterial conductivity measurement under the High Temperature High Pressure.
The prior art close with the present invention is a Chinese invention patent application, and name is called " being used for adamas opposed anvils of electrical quantity in-situ measurement and preparation method thereof ", and publication number is CN101078703.Electrode on the disclosed adamas opposed anvils is a Mo, and heat insulation layer of aluminum oxide and protective layer of alumina are housed.
Summary of the invention
The technical problem to be solved in the present invention is, overcome disadvantages of background technology, nano crystal introduction technology, diamond thin doping techniques and adamas opposed anvils superhigh pressure technique are combined, on the adamas opposed anvils, prepare boron doped diamond film electrode, created experiments of measuring technical method such as liquid corrosive liquid bulk conductivity under the superhigh-temperature and-pressure condition.
The electrode that is used for original position electrical measurement on the adamas opposed anvils of the present invention is at adamas the opposed anvils wherein surface deposition 2 of a diamond anvil (8) or 4 electrodes (1) of isolating mutually; The distribution of every strip electrode (1) be anvil face from diamond anvil (8) to the side, it is characterized in that described electrode (1) is the diamond film of doped with boron; Deposit adamas insulation course (2) on the electrode (1), adamas insulation course (2) covers on anvil face, side and the electrode (1) of diamond anvil (8), make electrode (1) exposed simultaneously in the termination of anvil face, the position of exposed termination is in the sample cavity (9) of adamas opposed anvils, make electrode (1) exposed simultaneously, be connected to contact conductor (5) on the exposed termination in the termination of side.
Diamond electrode has following advantage: one, the electrode conductance rate can be regulated according to the difference of boron doping concentration, to adapt to different samples.Two, boron-doped diamond film surface is a covalent structure, and very wide band gap and electrochemical window are arranged, and has high chemistry and electrochemical stability, and is corrosion-resistant.Three, the boron-doped diamond membrane electrode has carbon-carbon bond to link with adamas opposed anvils surface, can resist the destruction of the cross shear of anvil face edge, also can not produce the problem of fracture at the hyperpressure bottom electrode.Four, for the measurement of fluid sample, electric current is near zero at the bottom of the back of the body of diamond film electrode, this explanation is under equilibrium potential, almost there is not charged particle to shift between " electrode/solution " interface, the electric charge that flows to the interface is mainly used in the change interfacial structure, be a process of giving the charging of electrode space charged region, electrochemical reaction does not take place substantially.
The method for making that is used for the electrode of original position electrical measurement on the adamas opposed anvils of the present invention, the process that has electrode making, depositing diamond insulation course and receiving electrode to go between:
Described electrode manufacturing process is: the mixed liquid dipping of diamond anvil being put into acetone and alcohol is removed surface blot, take out the back deionized water rinsing, after the oven dry, put into vacuum chamber, utilize the surface deposition aluminum oxide film of magnetically controlled sputter method at diamond anvil; The diamond anvil that is coated with pellumina is taken out, smear one deck photoresist on its surface, utilize photoetching technique on the anvil face of diamond anvil and side, to carve the electrode isolation band, water-bath heating in phosphoric acid then makes the alumina layer that keeps the shape of electrode isolation band on the anvil face of diamond anvil and the side; Diamond anvil is immersed in the nano-diamond powder suspending liquid, take out oven dry, again diamond anvil is put into chemical vapor deposition unit and carry out the boron-doped diamond depositing of thin film; Be the corrosive liquid that mixes with sulfuric acid of 1: 1 nitric acid with volume ratio with the aluminium oxide at electrode isolation band place with and go up boron doped diamond film and erode, make on the anvil face of diamond anvil and the side to present diamond electrode;
The process of described depositing diamond insulation course is: utilize the outside deposition aluminum oxide film of magnetically controlled sputter method at diamond electrode and electrode isolation band, utilize the gluing photoetching and with phosphoric acid chemistry corroding method, keep the box-shaped aluminum oxide film in the anvil face center, big 20～100 μ m of the side ratio electrode isolation bandwidth of aluminum oxide film square, the place keeps an aluminum oxide film at the every strip electrode in diamond anvil side; Diamond anvil is put into chemical vapor deposition unit once more, be used as the deposition of diamond thin films of insulation course; The corrosive liquid that mixes with sulfuric acid with nitric acid with the aluminum oxide film of the reservation on diamond anvil anvil face and the side and on diamond thin remove, make the two ends of each electrode expose out;
The process of described receiving electrode lead-in wire is: copper wire is adhered on the exposed electrode in diamond anvil side with the silver slurry, solidifies 1.5～3 hours to reach the use desirable strength under 150 ℃ condition.
Aforesaid magnetically controlled sputter method deposition of aluminium oxide film, be as target with metallic aluminium, with throughput ratio be 30: 2.0～3.0 oxygen and argon gas as working gas, the pressure in the vacuum chamber remains on 0.8～1.2Pa, underlayer temperature remains on and carries out under 200～300 ℃.
Aforesaid electrode isolation band is to cover on the side of diamond anvil and the anvil face; The electrode isolation band is two, intersects mutually at the sample cavity place at diamond anvil anvil face center, becomes the crosshair shape.
Aforesaid when carrying out the boron-doped diamond depositing of thin film, make work gas with methane and hydrogen by throughput ratio 0.6～3:100, base reservoir temperature is under 750～850 ℃, deposits under 1-4KPa pressure; The thickness of boron-doped diamond film is preferably 0.5～2 μ m (approximately needing 20 to 60 minutes).During the unadulterated diamond thin of deposition, mode of deposition is identical with the boron-doped diamond depositing of thin film; Thickness of insulating layer is preferably 0.5～2 μ m.
When carrying out the boron doping, can do the boron source with solid boron powder, boric acid three formicesters, diborane etc.
The present invention is the achievement of finishing under project of national nature science fund project (40473034,10574055,50532020,10874053,50802033), the Department of Science and Technology's 973 projects (2005CB724404) and the programme support of innovation team of the Ministry of Education.The present invention utilizes film deposition techniques, nano crystal introduction technology, mask technique and means of photolithography that diamond thin microcircuit and adamas insulation course are integrated on the adamantine anvil face simultaneously, prevented the destruction of cross shear to electrode, improved the reliability of measuring microcircuit, overcome under the condition of high voltage sample to the corrosion of electrode, make the in site measurement to the electrical quantities that has the corrosivity sample under the high pressure become possibility, thereby widened the research field of electrical quantity in-situ measurement under the high pressure.
Description of drawings
Fig. 1 is the structural representation that is used for the electrode of original position electrical measurement on the adamas opposed anvils of the present invention.
Fig. 2 is the longitudinal diagram that has the adamas opposed anvils device of electrode of the present invention.
Fig. 3 is the manufacture craft process flow diagram of electrode of the present invention.
Embodiment
Among Fig. 1 and Fig. 2,1 is electrode, there are 4, the termination of every strip electrode 1 on the diamond anvil anvil face is box-shaped and all is positioned at the sample cavity 9 of diamond anvil, electrode tip 3 in the diamond anvil side is connected with the contact conductor 5 of copper wire, and the electrode 1 of boron-doped diamond film is covered by the insulation course 2 of diamond thin except that two ends; 2 is the adamas insulation course; 3 is the electrode tip in the diamond anvil side; 4 is the silver slurry; 5 is contact conductor, and contact conductor 5 is connected on the electrode tip 3 of diamond anvil side by silver slurry 4; 6 is alumina insulating layer; 7 is the T301 steel plate washer, and alumina insulating layer 6 is placed on it; 8 is diamond anvil, constitutes the adamas opposed anvils by two diamond anvils 8 up and down; 9 is sample cavity.
The sectional view of whole device as shown in Figure 2.
The first step: the mixed liquid dipping 20 minutes of diamond anvil being put into acetone and alcohol is used deionized water rinsing to remove surface blot after the taking-up.After the oven dry, put into vacuum chamber, utilize magnetically controlled sputter method with deposited aluminum oxide thin film at diamond surface.Shown in Fig. 3 (a).
In sputter procedure, adopt metallic aluminium as target, throughput ratio between 30: 2.0-3.0 oxygen and argon gas as working gas, the pressure in the vacuum chamber remains on 0.8-1.2Pa, underlayer temperature remains on 200 ℃-300 ℃.
Second step: the adamas that will be coated with pellumina takes out, evenly smear one deck photoresist on its surface, utilize photoetching technique on the adamas anvil face, to carve the crosshair shape, corrode (100 ℃ of water-bath heating in phosphoric acid) with corrosive liquid then, make to present crosshair on the anvil face, the cross hair width is 30-100 μ m.Shown in Fig. 3 (b).
Because the aluminium oxide that needs to keep the adamas side in photoetching process is with the protective money hard rock, so the process need manual mode is finished gluing.
The 3rd step: the diamond anvil that will have mask layer immerses in the nano-diamond powder suspending liquid, takes out under 100 ℃ of conditions again and dries, and so repeats five times.Shown in Fig. 3 (c).
This step purpose is to make diamond surface adhere to one deck Nano diamond particle, and these particles help next step as nucleus and deposit high boron doped diamond film.
The 4th step: will put into the chemical vapor deposition (CVD) device with the diamond anvil of nano-diamond powder, and carry out high boron-doped diamond depositing of thin film.Keeping base reservoir temperature in the deposition process is 750 ℃-850 ℃, and the thickness of boron-doped diamond film is 500nm-2 μ m.Shown in Fig. 3 (d).
Should note in this process preventing that the diamond film that deposits is blocked up, make diamond film on the crosshair and cross hair be linked to be film, influence the corrosion in the 5th step with the adamas of exterior domain.
The 5th step: with the alumina layer at the crosshair place on anvil face and the side with and on boron doped diamond film erode with corrosive liquid (volume ratio is the nitric acid of 1:1 and the mixed liquor of sulfuric acid), make to present diamond electrode on the anvil face.Shown in Fig. 3 (e).
The 6th step: repeat first step step, utilize the method for photoetching and chemical corrosion to stay four aluminium oxide squares on aluminium oxide square in anvil face center and the side, wherein Zhong Yang the square length of side is 50-160 μ m.Four aluminium oxide square sizes on the side are not done requirement.Shown in Fig. 3 (f).
The 7th step: the electrode of handling well in the 6th step is put into chemical vapor deposition unit once more, carry out not doped diamond depositing of thin film.The diamond film that is deposited is used as insulation course, and the deposit thickness of film is 500nm-2 μ m.Shown in Fig. 3 (g).
Should note equally in this process preventing that the diamond film that deposits is blocked up,, and influence next step corrosion in order to avoid the diamond film on the crosshair links to each other with the adamas of cross hair surface with exterior domain.
The 8th step: repeat the 5th suddenly step by step, five aluminium oxide squares on the adamas anvil face and the diamond thin on it thereof are removed, make electrode expose out with corrosive liquid.Shown in Fig. 3 (h).
The 9th step: copper wire that will be very thin has on the exposed electrode with four sides that the silver slurry is adhered to diamond anvil, solidifying about two hours under 150 ℃ the condition, to reach the use desirable strength.Shown in Fig. 3 (i).
The manufacture craft process that two strip electrodes are arranged on embodiment 3 diamond anvils of the present invention.
Whole technological process is identical with embodiment 2.Just utilize photoetching technique to make a strip electrode isolation strip in second step, the sample cavity at anvil face center is passed through again to the relative another side of diamond anvil from a side of diamond anvil in this strip electrode isolation strip; The 6th step was to leave two aluminium oxide squares on the diamond anvil side.
Claims (4)
1, a kind of electrode that is used for original position electrical measurement on the adamas opposed anvils is at adamas the opposed anvils wherein surface deposition 2 of a diamond anvil (8) or 4 electrodes (1) of isolating mutually; The distribution of every strip electrode (1) be anvil face from diamond anvil (8) to the side, it is characterized in that described electrode (1) is the diamond film of doped with boron; Deposit adamas insulation course (2) on the electrode (1), adamas insulation course (2) covers on anvil face, side and the electrode (1) of diamond anvil (8), make electrode (1) exposed simultaneously in the termination of anvil face, the position of exposed termination is in the sample cavity (9) of adamas opposed anvils, make electrode (1) exposed simultaneously, be connected to contact conductor (5) on the exposed termination in the termination of side.
2, a kind of method for making that is used for the electrode of original position electrical measurement on the adamas opposed anvils of claim 1, the process that has electrode making, depositing diamond insulation course and receiving electrode to go between:
Described electrode manufacturing process is: the mixed liquid dipping of diamond anvil being put into acetone and alcohol is removed surface blot, take out the back deionized water rinsing, after the oven dry, put into vacuum chamber, utilize the surface deposition aluminum oxide film of magnetically controlled sputter method at diamond anvil; The diamond anvil that is coated with pellumina is taken out, smear one deck photoresist on its surface, utilize photoetching technique on the anvil face of diamond anvil and side, to carve the electrode isolation band, water-bath heating in phosphoric acid then makes the alumina layer that keeps the shape of electrode isolation band on the anvil face of diamond anvil and the side; Diamond anvil is immersed in the nano-diamond powder suspending liquid, take out oven dry, again diamond anvil is put into chemical vapor deposition unit and carry out the boron-doped diamond depositing of thin film; Be the corrosive liquid that mixes with sulfuric acid of 1: 1 nitric acid with volume ratio with the aluminium oxide at electrode isolation band place with and go up boron doped diamond film and erode, make on the anvil face of diamond anvil and the side to present diamond electrode;
The process of described depositing diamond insulation course is: utilize the outside deposition aluminum oxide film of magnetically controlled sputter method at diamond electrode and electrode isolation band, utilize the gluing photoetching and with phosphoric acid chemistry corroding method, keep the box-shaped aluminum oxide film in the anvil face center, big 20～100 μ m of the side ratio electrode isolation bandwidth of aluminum oxide film square, the place keeps an aluminum oxide film at the every strip electrode in diamond anvil side; Diamond anvil is put into chemical vapor deposition unit once more, be used as the deposition of diamond thin films of insulation course; The corrosive liquid that mixes with sulfuric acid with nitric acid with the aluminum oxide film of the reservation on diamond anvil anvil face and the side and on diamond thin remove, make the two ends of each electrode expose out;
The process of described receiving electrode lead-in wire is: copper wire is adhered on the exposed electrode in diamond anvil side with the silver slurry, solidifies 1.5～3 hours to reach the use desirable strength under 150 ℃ condition.
According to the described method for making that is used for the electrode of original position electrical measurement on the adamas opposed anvils of claim 2, it is characterized in that 3, described electrode isolation band is to cover on the side of diamond anvil and the anvil face; The electrode isolation band is two, intersects at the sample cavity place at diamond anvil anvil face center, becomes the crosshair shape.
4, according to claim 2 or the 3 described method for makings that are used for the electrode of original position electrical measurement on the adamas opposed anvils, it is characterized in that, described magnetically controlled sputter method deposition of aluminium oxide film, be as target with metallic aluminium, with throughput ratio is that 30: 2.0～3.0 oxygen and argon gas are as working gas, pressure in the vacuum chamber remains on 0.8～1.2Pa, and underlayer temperature remains on and carries out under 200～300 ℃.
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| CN102200480A (en) * | 2011-03-23 | 2011-09-28 | 吉林大学 | In-situ temperature measuring thermocouple on diamond anvil cell and preparation method thereof |
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| US5594546A (en) * | 1995-03-28 | 1997-01-14 | The Regents Of The University Of California | Diamond anvil cell for spectroscopic investigation of materials at high temperature, high pressure and shear |
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